For the first time, we report a Two Dimensional Phase Transfer Reaction (2DPTR) between the three different phases of 2D nanosheets and their applications in catalysis and hydrogen evolution. Plasmonic two-dimensional (2D) nanomaterials have created a niche for themselves in a variety of applications due to their unique and tunable optical properties. In the present work, we report a simple method for the synthesis of three different phases of the 2D vanadium oxide nanosheets to convert to each other at room temperature (amorphous, nanoflakes and nanotriangles). We developed a two-step method that first involves probe ultrasonication to mediate the synthesis of 2D vanadium oxide nanoflakes (VNFs) at room temperature and secondly, their phase transformation to VNTs using hydrogen peroxide or Isopropyl Alcohol (IPA) as the phase transfer reagents. 2D VNTs have been studied for morphological, structural, and optical properties by using a variety of instruments, including TEM, UV–Vis, EPR, RAMAN, and XPS. Thus, after treatment with hydrochloric acid (HCl), the 2D vanadium oxide nanoflakes are easily converted to the 2D amorphous nanosheets (Vam) which then regain crystallinity in the form of VNTs after the addition of Hydrogen peroxide or IPA, with a plasmonic peak around 450 nm. Oxygen vacancies are created in the VNFs, after treatment with HCl, which results in the crystal lattice breakdown. These oxygen vacancies were filled up again when the nanoflakes were treated with hydrogen peroxide or IPA and then resulted in the formation of VNTs. The UV–vis spectroscopy was performed with different addition of concentrations of H2O2, the limit of detection 34.1 µM and linear range 0 to 1000 µM found. Also, a selectivity study proved H2O2 in these 2D VNTs. Vam and VNT also showed effective photocatalytic activity against KMnO4 which is a strong oxidizing reagent used in water treatment. The synthesis and plasmonic nature of the 2D VNTs and the photocatalytic activity of Vam and VNT present in this study is a pioneer report for these novel 2D nanomaterials and they can be further explored with many possibilities in many fields including sensing, catalysis, energy, biomedicine, and many other significant applications in the near future.